Citation: ZHU Dingji, LU Minping, HUANG Kejian, ZHOU Zhe, LIN Cuiwu, YANG Ning, LIU Xiaofeng, QIAO Wentao, LI Lu, HUANG Xiaoqing. Simultaneous determination of seven aconitum alkaloids in biological samples by liquid chromatography-linear ion trap multistage mass spectrometry coupled with on-line solid phase extraction[J]. Chinese Journal of Chromatography, ;2016, 34(3): 249-257. doi: 10.3724/SP.J.1123.2015.10044 shu

Simultaneous determination of seven aconitum alkaloids in biological samples by liquid chromatography-linear ion trap multistage mass spectrometry coupled with on-line solid phase extraction

ZHU Dingji ¹ ,
LU Minping ² ,
HUANG Kejian ^3,, ,
ZHOU Zhe ⁴ ,
LIN Cuiwu ² ,
YANG Ning ³ ,
LIU Xiaofeng ³ ,
QIAO Wentao ³ ,
LI Lu ³ ,
HUANG Xiaoqing ³

1.
1. Guangxi Zhuang Autonomous Region Academy for the Prevention and Treatment of Occupational Diseases, Nanning 530021, China;
2.
2. School of Chemistry and Chemical Engineering, Guangxi University, Nanning 530004, China;
3.
3. Evidence Identification Center, Guangxi Zhuang Autonomous Region Public Security Department, Nanning 530012, China;
4.
4. Thermo Fisher Scientific (China) Co., Ltd., Shanghai 201206, China

Corresponding author: HUANG Kejian,
Received Date: 29 October 2015

An analytical method has been developed for the simultaneous determination of seven aconitum alkaloids in biological samples by liquid chromatography-linear ion trap multistage mass spectrometry (LC-LIT/MSⁿ) coupled with on-line solid phase extraction (on-line SPE). Mass fragmentation regularities of the seven aconitum alkaloids are discussed and summarized according to the analysis of their MSⁿ fragments. The samples were treated with acetonitrile for protein precipitation, followed by dilution and centrifugation. The resulting solution was injected into the LC system directly and processed by Waters Oasis^® HLB on-line SPE column for enrichment and purification. Chromatographic separation was performed on an Accucore C18 column using mobile phases of 0.01 mol/L ammonium acetate aqueous solution and methanol (both containing 0.1%(v/v) formic acid) for gradient elution. The analytes were detected in consecutive reaction monitoring (CRM) mode through positive electrospray ionization (ESI⁺). The calibration curves of the analytes within the investigated mass concentration ranges were fitted by second-order equations weighted 1/x, with r² ranging from 0.9991 to 0.9999. The method detection limits were 0.02-0.60 ng/mL for whole blood and urine, 0.02-0.40 ng/g for liver tissue. The recoveries at three spiked levels were within 91.1%-104.7%for all the analytes, with 0.2%-10.7%of intra-day RSDs and 1.0%-13.7%of inter-day RSDs (n=6). The established method is simple, accurate, and sensitive for rapid determination of the seven aconitum alkaloids in biological samples.
1. [1]
  [1] Qiu K, Wu H, Wang H Y. Chinese Pharmaceutical Journal, 2010, 45(8): 633 邱葵, 吴华, 王鹤尧. 中国药学杂志, 2010, 45(8): 633
2. [2]
  [2] Wang Z Q, Jing X, Zeng R, et al. Chinese Journal of Clinical Pharmacology and Therapeutics, 2012, 17(4): 371 王志琪, 景贤, 曾嵘, 等. 中国临床药理学与治疗学, 2012, 17(4): 371
3. [3]
  [3] Wang Z H, He Y, Zhang J Z, et al. Chinese Journal of Forensic Medicine, 2003, 18(3): 145 王朝虹, 何毅, 张继宗, 等. 中国法医学杂志, 2003, 18(3): 145
4. [4]
  [4] Guo D, Lin J Y, Zhou C Q, et al. Strait Pharmaceutical Journal, 2011, 23(12): 32 郭丹, 林静瑜, 周春权, 等. 海峡药学, 2011, 23(12): 32
5. [5]
  [5] Zhang X Y, Cai X X, Lin X Y, et al. Journal of Food Safety and Quality, 2013, 4(3): 715 张秀尧, 蔡欣欣, 林学尧, 等. 食品安全质量检测学报, 2013, 4(3): 715
6. [6]
  [6] Yang C P, Liao S, Zhang T H, et al. International Journal of Pharmaceutical Research, 2012, 39(3): 256 杨翠平, 廖沙, 张天宏, 等. 国际药学研究杂志, 2012, 39(3): 256
7. [7]
  [7] Liu J J, Li Q, Yin Y D, et al. J Sep Sci, 2014, 37(1/2): 171
8. [8]
  [8] Zhang P P, Zhang F C, Wang Z H, et al. Chinese Journal of Chromatography, 2013, 31(3): 211 张盼盼, 张福成, 王朝虹, 等. 色谱, 2013, 31(3): 211
9. [9]
  [9] Wu J, Shen H, Zhu L Y, et al. Chinese Journal of Hospital Pharmacy, 2011, 31(14): 1162 武洁, 沈红, 朱玲英, 等. 中国医院药学杂志, 2011, 31(14): 1162
10. [10]
  [10] Liu W, Shen M, Wu H J, et al. Chinese Journal of Pharmaceutical Analysis, 2009, 29(12): 2023 刘伟, 沈敏, 吴何坚, 等. 药物分析杂志, 2009, 29(12): 2023
11. [11]
  [11] Wang H L, Dong L, Xu D F, et al. Journal of Liaoning University of Traditional Chinese Medicine, 2010, 12(1): 191 王海龙, 董雷, 许大方, 等. 辽宁中医药大学学报, 2010, 12(1): 191
12. [12]
  [12] Xiong X T, Wu H Q, Huang X L. Chinese Journal of Analytical Chemistry, 2009, 37(10): 1433 熊小婷, 吴惠勤, 黄晓兰. 分析化学, 2009, 37(10): 1433
13. [13]
  [13] Ng S W, Ching C K, Chan A Y W, et al. J Chromatogr B, 2013, 942/943: 63
14. [14]
  [14] Du Z X, Sun S Q. Journal of Instrumental Analysis, 2007, 26(Suppl): 61 杜振霞, 孙姝琦. 分析测试学报, 2007, 26(增刊): 61
15. [15]
  [15] Usui K, Hayashizaki Y, Hashiyada M, et al. Leg Med, 2012, 14(3): 126
16. [16]
  [16] Qiu P H, Chen X H, Chen X, et al. J Chromatogr B, 2008, 875(2): 471
17. [17]
  [17] Zhang H G, Sun Y, Duan M Y, et al. Toxicon, 2005, 46(5): 500
18. [18]
  [18] Wang Z H, Wang Z P, Wen J, et al. J Pharm Biomed Anal, 2007, 45(1): 145
19. [19]
  [19] Hayashida M, Hayakawa H, Wada K, et al. Leg Med, 2003, 5(Suppl 1): S101
20. [20]
  [20] Huang K J, Lu M P, Zhou Z, et al. Chinese Journal of Chromatography, 2015, 33(7): 691 黄克建, 卢敏萍, 周哲, 等. 色谱, 2015, 33(7): 691
21. [21]
  [21] Li X, Zhang Y Q, Ai L F, et al. Chinese Journal of Chromatography, 2015, 33(6): 590 李欣, 张瑶琴, 艾连峰, 等. 色谱, 2015, 33(6): 590
22. [22]
  [22] Duan Y S, Wang B L, Ai L F, et al. Chinese Journal of Chromatography, 2014, 32(6): 647 段永生, 王炳玲, 艾连峰, 等. 色谱, 2014, 32(6): 647
23. [23]
  [23] Chen J, Liu Z J, An B C, et al. Chinese Journal of Chromatography, 2012, 30(10): 1068 陈静, 刘召金, 安保超, 等. 色谱, 2012, 30(10): 1068
24. [24]
  [24] Chen J H, Lee C Y, Liau B C, et al. J Pharm Biomed Anal, 2008, 48(4): 1105
25. [25]
  [25] US EPA. Title 40: Protection of Environment; Part 136-Guidelines Establishing Test Procedures for the Analysis of Pollutants; Appendix B to Part 136-Definition and Procedure for the Determination of the Method Detection Limit-Revision 1.11. [2015-12-21]. http://www.ecfr.gov/cgi-bin/text-idx?SID=aca7e8a173fd9625b56ff91d6a326994&mc=true&node =ap40.23.136_17.b&rgn=div9
1. [1]
  Yanhui Zhong , Ran Wang , Zian Lin . Analysis of Halogenated Quinone Compounds in Environmental Water by Dispersive Solid-Phase Extraction with Liquid Chromatography-Triple Quadrupole Mass Spectrometry. University Chemistry, 2024, 39(11): 296-303. doi: 10.12461/PKU.DXHX202402017
2. [2]
  Yurong Tang , Yunren Shi , Yi Xu , Bo Qin , Yanqin Xu , Yunfei Cai . Innovative Experiment and Course Transformation Practice of Visible-Light-Mediated Photocatalytic Synthesis of Isoquinolinone. University Chemistry, 2024, 39(5): 296-306. doi: 10.3866/PKU.DXHX202311087
3. [3]
  Zunxiang Zeng , Yuling Hu , Yufei Hu , Hua Xiao . Analysis of Plant Essential Oils by Supercritical CO₂Extraction with Gas Chromatography-Mass Spectrometry: An Instrumental Analysis Comprehensive Experiment Teaching Reform. University Chemistry, 2024, 39(3): 274-282. doi: 10.3866/PKU.DXHX202309069
4. [4]
  Tianlong Zhang , Rongling Zhang , Hongsheng Tang , Yan Li , Hua Li . Online Monitoring and Mechanistic Analysis of 3,5-diamino-1,2,4-triazole (DAT) Synthesis via Raman Spectroscopy: A Recommendation for a Comprehensive Instrumental Analysis Experiment. University Chemistry, 2024, 39(6): 303-311. doi: 10.3866/PKU.DXHX202312006
5. [5]
  Zhibei Qu , Changxin Wang , Lei Li , Jiaze Li , Jun Zhang . Organoid-on-a-Chip for Drug Screening and the Inherent Biochemistry Principles. University Chemistry, 2024, 39(7): 278-286. doi: 10.3866/PKU.DXHX202311039
6. [6]
  Xin MA , Ya SUN , Na SUN , Qian KANG , Jiajia ZHANG , Ruitao ZHU , Xiaoli GAO . A Tb₂ complex based on polydentate Schiff base: Crystal structure, fluorescence properties, and biological activity. Chinese Journal of Inorganic Chemistry, 2024, 40(7): 1347-1356. doi: 10.11862/CJIC.20230357
7. [7]
  Jinlong YAN , Weina WU , Yuan WANG . A simple Schiff base probe for the fluorescent turn-on detection of hypochlorite and its biological imaging application. Chinese Journal of Inorganic Chemistry, 2024, 40(9): 1653-1660. doi: 10.11862/CJIC.20240154
8. [8]
  . . Chinese Journal of Inorganic Chemistry, 2024, 40(12): 0-0.
9. [9]
  Feiya Cao , Qixin Wang , Pu Li , Zhirong Xing , Ziyu Song , Heng Zhang , Zhibin Zhou , Wenfang Feng . Magnesium-Ion Conducting Electrolyte Based on Grignard Reaction: Synthesis and Properties. University Chemistry, 2024, 39(3): 359-368. doi: 10.3866/PKU.DXHX202308094
10. [10]
  Gaoyan Chen , Chaoyue Wang , Juanjuan Gao , Junke Wang , Yingxiao Zong , Kin Shing Chan . Heart to Heart: Exploring Cardiac CT. University Chemistry, 2024, 39(9): 146-150. doi: 10.12461/PKU.DXHX202402011
11. [11]
  Mingyang Men , Jinghua Wu , Gaozhan Liu , Jing Zhang , Nini Zhang , Xiayin Yao . 液相法制备硫化物固体电解质及其在全固态锂电池中的应用. Acta Physico-Chimica Sinica, 2025, 41(1): 2309019-. doi: 10.3866/PKU.WHXB202309019
12. [12]
  Haitang WANG , Yanni LING , Xiaqing MA , Yuxin CHEN , Rui ZHANG , Keyi WANG , Ying ZHANG , Wenmin WANG . Construction, crystal structures, and biological activities of two Ln^Ⅲ₃ complexes. Chinese Journal of Inorganic Chemistry, 2024, 40(8): 1474-1482. doi: 10.11862/CJIC.20240188
13. [13]
  Xiaowei TANG , Shiquan XIAO , Jingwen SUN , Yu ZHU , Xiaoting CHEN , Haiyan ZHANG . A zinc complex for the detection of anthrax biomarker. Chinese Journal of Inorganic Chemistry, 2024, 40(10): 1850-1860. doi: 10.11862/CJIC.20240173
14. [14]
  Jianfeng Yan , Yating Xiao , Xin Zuo , Caixia Lin , Yaofeng Yuan . Comprehensive Chemistry Experimental Design of Ferrocenylphenyl Derivatives. University Chemistry, 2024, 39(4): 329-337. doi: 10.3866/PKU.DXHX202310005
15. [15]
  Dan Li , Hui Xin , Xiaofeng Yi . Comprehensive Experimental Design on Ni-based Catalyst for Biofuel Production. University Chemistry, 2024, 39(8): 204-211. doi: 10.3866/PKU.DXHX202312046
16. [16]
  Yang Liu , Peng Chen , Lei Liu . Chemistry “101 Plan”: Design and Construction of Chemical Biology Textbook. University Chemistry, 2024, 39(10): 45-51. doi: 10.12461/PKU.DXHX202407085
17. [17]
  Tianyu Feng , Guifang Jia , Peng Zou , Jun Huang , Zhanxia Lü , Zhen Gao , Chu Wang . Construction of the Chemistry Biology Experiment Course in the Chemistry “101 Program”. University Chemistry, 2024, 39(10): 69-77. doi: 10.12461/PKU.DXHX202409002
18. [18]
  Zhaoxin LI , Ruibo WEI , Min ZHANG , Zefeng WANG , Jing ZHENG , Jianbo LIU . Advancements in the construction of inorganic protocells and their cell mimic and bio-catalytical applications. Chinese Journal of Inorganic Chemistry, 2024, 40(12): 2286-2302. doi: 10.11862/CJIC.20240235
19. [19]
  Jinghan ZHANG , Guanying CHEN . Progress in the application of rare-earth-doped upconversion nanoprobes in biological detection. Chinese Journal of Inorganic Chemistry, 2024, 40(12): 2335-2355. doi: 10.11862/CJIC.20240249
20. [20]
  Chongjing Liu , Yujian Xia , Pengjun Zhang , Shiqiang Wei , Dengfeng Cao , Beibei Sheng , Yongheng Chu , Shuangming Chen , Li Song , Xiaosong Liu . Understanding Solid-Gas and Solid-Liquid Interfaces through Near Ambient Pressure X-Ray Photoelectron Spectroscopy. Acta Physico-Chimica Sinica, 2025, 41(2): 100013-. doi: 10.3866/PKU.WHXB202309036

Get Citation

PDF

XML

Metrics

PDF Downloads(0)
Abstract views(588)
HTML views(16)

通讯作者: 陈斌, bchen63@163.com

1.
沈阳化工大学材料科学与工程学院沈阳 110142